CN108841158A - A kind of graphene-foaming polycarbonate composite material and preparation method thereof - Google Patents
A kind of graphene-foaming polycarbonate composite material and preparation method thereof Download PDFInfo
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- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 46
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 45
- 238000005187 foaming Methods 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 70
- 239000004088 foaming agent Substances 0.000 claims abstract description 25
- 239000006260 foam Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 28
- 238000000889 atomisation Methods 0.000 claims description 26
- 229910052760 oxygen Inorganic materials 0.000 claims description 25
- 239000001301 oxygen Substances 0.000 claims description 25
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 22
- 239000002356 single layer Substances 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 235000021355 Stearic acid Nutrition 0.000 claims description 12
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 12
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 12
- 239000008117 stearic acid Substances 0.000 claims description 12
- 239000011787 zinc oxide Substances 0.000 claims description 12
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 abstract description 12
- 239000004425 Makrolon Substances 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 230000004069 differentiation Effects 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 19
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- -1 oxygen Graphite alkene Chemical class 0.000 description 6
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 206010000269 abscess Diseases 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- OKIRBHVFJGXOIS-UHFFFAOYSA-N 1,2-di(propan-2-yl)benzene Chemical compound CC(C)C1=CC=CC=C1C(C)C OKIRBHVFJGXOIS-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K5/00—Use of organic ingredients
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/14—Peroxides
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Abstract
The invention discloses a kind of graphene-foaming polycarbonate composite materials and preparation method thereof, it is added in polycarbonate and is uniformly mixed by the foaming agent and graphene oxide microballoon that will premix, after first step low-temp foaming, polycarbonate inner forms hole, graphene oxide microballoon is distributed in inside hole, again after second step foams, foaming agent further decomposes so that hole is able to continued growth, and the graphene oxide microballoon in hole is expanded and is restored, it is gradually filled with hole, finally obtains the foaming makrolon material of porous graphene filling.Graphene is filled in polycarbonate hole, plays the role of support and energy absorption, is greatly enhanced the intensity and elasticity of foamed material, is obtained differentiation foamed material.This method is simple and easy, and the addition of graphene oxide without influence, can assign material new function original preparation process after promoting material foundation performance, has broad prospect of application.
Description
Technical field
The invention belongs to field of compound material more particularly to a kind of graphene-foaming polycarbonate composite material and its systems
Preparation Method.
Background technique
Polycarbonate is a kind of unformed thermoplastic, it has transparent, high heat distortion temperature and good impact
The characteristics such as intensity, the heat-insulated of polycarbonate, sound insulation value are good, and conductivity and thermal coefficient are low, have stronger luminous reflectanc
Many advantages, such as, it up to the present can possess so more advantages simultaneously there are no Other Engineering plastics.It is frequently utilized for making
Make CD, gear, pipe fitting, electric power tool shell, electrical instrumentation part and shell, shield and instrument board etc..But it has
One very big disadvantage is exactly easily to cause stress cracking, and its microporous foam is enable preferably to solve this problem, mainly because
For the abscess-size in microcellular foam be less than foamed plastics inside defect, the presence of this small abscess not but not drop
The mechanical strength of low foamed plastics can be present such that unborn Crack Tip in foamed plastics due to these micropores instead
End passivation, extends under stress, therefore improve polycarbonate to be beneficial to prevent existing crackle in material
The mechanical property of foamed plastics.Polycarbonate can not only reduce density, save the cost, and its impact flexibility after microporous foam
Also the shortcomings that being improved, effectively improving its easy stress cracking.
Graphene is a kind of two-dimentional carbon material with monoatomic layer thickness, has low-density, high mechanical strength, heat
Conductance and conductivity and excellent corrosion resistance, and it is good with the compatibility of high molecular material, it can be used as the increasing of high molecular material
Strong body uses.The performance indexes of material can be obviously improved by (being lower than 1%) under extremely low additive amount, have wide city
Field prospect.
The present invention utilizes the thermal instability of graphene oxide microballoon, and graphene oxide microballoon and foaming agent is total in advance
It is mixed, it adds in the mixed system of polycarbonate and other auxiliary agents.In first segment foaming, foaming agent first decomposites gas poly-
Hole is formed in carbonic ester, and graphene oxide microballoon then stays in these holes.After temperature is further promoted, on the one hand send out
Infusion decomposes completely, and hole growth is promoted to expand, and the oxygen-containing group on another aspect graphene oxide sheet surface decomposes, so that oxidation
Volume expansion occurs for graphene microballoon, to gradually be filled into the hole of polycarbonate, forms supporting network structure.Finally make
The mechanical property for obtaining composite material is obviously improved, and due to the presence of graphene, so that stability of the composite foam to light, heat
Obtain a degree of promotion
Summary of the invention
The purpose of the present invention is aiming at the shortcomings of the prior art, provide a kind of graphene-foaming polycarbonate composite material
And preparation method thereof.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of preparation method of graphene-foaming polycarbonate composite material, includes the following steps：
(1) will be dry having a size of 1~50 micron of single-layer graphene oxide dispersion liquid by atomization drying method, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio are 3~6.
(2) 1~10 mass parts graphene oxide microballoon for obtaining step (1) mixes with 1~6 mass parts foaming agent
It is even.
(3) by 100 mass parts polycarbonate and 0.1~0.6 part of stearic acid, 0.3~1 part of cumyl peroxide, 0.6~
1 part of zinc oxide, which is added in mixer, carries out mixing, and temperature is 85~100 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100~110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3~10 minutes at 120~135 DEG C, is warming up to 136
~300 DEG C are foamed 8~30 minutes.
Further, the atomization drying temperature of the step (1) is 130~200 DEG C.
Further, the foaming agent of the step (2) is AC foaming agent, and decomposition temperature is 130~140 DEG C.
The beneficial effects of the present invention are：
(1) using the technique of two steps foaming, graphene film is overlapped to form the hole that porous network is filled in foaming polycarbonate
Among.Wherein, form primary hole configurations in the first foaming stages, graphene oxide microballoon be selectively present in these holes it
In.Graphene oxide is set to be reduced to graphene in the oxygen-containing functional group fast eliminating of the second foaming stages surface of graphene oxide,
Graphene oxide microballoon occurs volume expansion and is full of hole, while foaming agent further decomposes, and forms porous structure.
(2) graphene film is mutually lapped to form network structure in hole, since direction has height to graphene film in face
Strong high mould performance has excellent flexibility in normal direction, thus after forming network, the stretching that can not only promote foaming polycarbonate is strong
Degree and hardness, while its stability to light, heat can be promoted.
To sum up, the foaming polycarbonate obtained using this method not only has outstanding representation in mechanical property, in photo-thermal
Also there is broad prospect of application in the multifunctionality such as stability, suitable for modern multi-functional, mass production, simple and easy requirement.
Specific embodiment
Graphene-foaming polycarbonate composite material method is prepared to include the following steps：
(1) will be dry having a size of 1~50 micron of single-layer graphene oxide dispersion liquid by atomization drying method, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio are 3~6.The atomization drying temperature is 130~200 DEG C.(2) by step (1) obtain 1~
10 mass parts graphene oxide microballoons are uniformly mixed with 1~6 mass parts foaming agent.The foaming agent is AC foaming agent, decomposes temperature
Degree is 130~140 DEG C.(3) by 100 mass parts polycarbonate and 0.1~0.6 part of stearic acid, 0.3~1 part of peroxidating diisopropyl
Benzene, 0.6~1 part of zinc oxide, which is added in mixer, carries out mixing, and temperature is 85~100 DEG C.(4) by the product and step of step (3)
Suddenly mixer is added in the product of (2) together, in 100~110 DEG C of mixings.(5) mold is added in the product for obtaining step (4),
It foams 3~10 minutes at 120~135 DEG C, is warming up to 136~300 DEG C and foams 8~30 minutes.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment belong to protection scope of the present invention.
Embodiment 1：
(1) will be dry having a size of 1~10 micron of single-layer graphene oxide dispersion liquid by atomization drying method, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 130 DEG C.
(2) the 1 mass parts graphene oxide microballoon that step (1) obtains is uniformly mixed with 1 mass parts AC foaming agent.
(3) by 100 mass parts polycarbonate and 0.1 part of stearic acid, 0.3 part of cumyl peroxide, 0.6 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 85 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 10 minutes at 120 DEG C, is warming up to 300 DEG C and foams 8 points
Clock.
Through above step, graphene-foaming polycarbonate composite material is obtained, specific performance is as shown in table 1.
Embodiment 2：
(1) will be dry having a size of 10~20 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 4.Atomization drying temperature is 145 DEG C.
(2) the 3 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 3 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.3 part of stearic acid, 0.6 part of cumyl peroxide, 0.8 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 90 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 105 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3 minutes at 135 DEG C, is warming up to 136 DEG C and foams 30 points
Clock.
Through above step, graphene-foaming polycarbonate composite material is obtained, specific performance is as shown in table 1.
Embodiment 3：
(1) will be dry having a size of 20~30 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 5.Atomization drying temperature is 180 DEG C.
(2) the 5 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 4 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.6 part of stearic acid, 1.0 parts of cumyl peroxides, 1.0 parts of zinc oxide add
Enter and carry out mixing in mixer, temperature is 100 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 7 minutes at 130 DEG C, is warming up to 280 DEG C and foams 12 points
Clock.
Through above step, graphene-foaming polycarbonate composite material is obtained, specific performance is as shown in table 1.
Embodiment 4：
(1) will be dry having a size of 40~50 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 6.Atomization drying temperature is 200 DEG C.
(2) the 1 mass parts graphene oxide microballoon that step (1) obtains is uniformly mixed with 5 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.4 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 98 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 6 minutes at 132 DEG C, is warming up to 280 DEG C and foams 9 points
Clock.
Through above step, graphene-foaming polycarbonate composite material is obtained, specific performance is as shown in table 1.
Embodiment 5：
(1) will be dry having a size of 40~50 microns of single-layer graphene oxide dispersion liquid by atomization drying method, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 5.Atomization drying temperature is 150 DEG C.
(2) the 10 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 6 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.2 part of stearic acid, 0.8 part of cumyl peroxide, 0.9 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 100 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 6 minutes at 126 DEG C, is warming up to 240 DEG C and foams 15 points
Clock.
Through above step, graphene-foaming polycarbonate composite material is obtained, specific performance is as shown in table 1.
Comparative example 1：Graphene oxide microballoon preparation foaming polycarbonate is not added.
Comparative example 2：
(1) by atomization drying method that 0.1~5 micron of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 130 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 3：
(1) by atomization drying method that 100~300 microns of size of single-layer graphene oxide dispersion liquid is dry, obtain oxygen
Graphite alkene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 130 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 4：
(1) by atomization drying method that 40~50 microns of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 10.Atomization drying temperature is 250 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 5：
(1) by atomization drying method that 40~50 microns of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 250 DEG C.
(2) the 0.5 mass parts graphene oxide microballoon that step (1) obtains is uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 100 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 6：
(1) by atomization drying method that 40~50 microns of size of single-layer graphene oxide dispersion liquid is dry, it is aoxidized
Graphene microballoon, carbon-to-oxygen ratio 3.Atomization drying temperature is 250 DEG C.
(2) the 20 mass parts graphene oxide microballoons that step (1) obtains are uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 100 DEG C.
, with embodiment 1, specific performance is as shown in table 1 for remaining.
Comparative example 7：
(1) being dried by air blast will be dry having a size of 1~5 micron of single-layer graphene oxide dispersion liquid, obtains oxidation stone
Black alkene dry powder, carbon-to-oxygen ratio 10.Drying temperature is 180 DEG C.
(2) the 5 mass parts graphene oxide dry powder that step (1) obtains are uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 100 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3 minutes at 135 DEG C, is warming up to 165 DEG C and foams 5 points
Clock
Through above step, graphene-foaming polycarbonate composite material is obtained, specific performance is as shown in table 1.
Comparative example 8：
(1) being dried by air blast will be dry having a size of 1~5 micron of single-layer graphene oxide dispersion liquid, obtains oxidation stone
Black alkene dry powder, carbon-to-oxygen ratio 3.Drying temperature is 180 DEG C.
(2) the 5 mass parts graphene oxide dry powder that step (1) obtains are uniformly mixed with 2 mass parts AC foaming agents.
(3) by 100 mass parts polycarbonate and 0.3 part of stearic acid, 0.5 part of cumyl peroxide, 0.7 part of zinc oxide adds
Enter and carry out mixing in mixer, temperature is 100 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 20 minutes at 200 DEG C.
Through above step, graphene-foaming polycarbonate composite material is obtained, specific performance is as shown in table 1.
1 embodiment of table and comparative example relevant parameter and product property
It can be seen that the graphene oxide ruler at 1~50 micron from the comparison of embodiment 1,2,3 and comparative example 1,2,3
The excellent combination property of foaming polycarbonate in very little range.When lamella size is too small, graphene film can not effectively play enhancing effect
Fruit (comparative example 2), and it is oversized when, the contact area between graphene oxide sheet increases, and leads to the suction between graphene oxide sheet
Gravitation increases, and can not effectively expand in a heated state, and final product is still that spherical graphite alkene particle is present among hole, rises
Less than reinforcing effect (comparative example 3).
As can be seen that the control of graphene oxide carbon-to-oxygen ratio is relatively more reasonable 3~6 from embodiment Isosorbide-5-Nitrae and comparative example 4, carbon
Oxygen than it is excessively high when, surface group quantity is few, it is difficult to make graphene oxide microsphere expansion (comparative example 4).Carbon-to-oxygen ratio is difficult lower than 3 comparisons
Large-sized graphene oxide is obtained, therefore is not discussed here.
From embodiment Isosorbide-5-Nitrae, 5 and comparative example 5,6 in as can be seen that graphene oxide additive amount between 1~10% most
It is reasonable.When additive amount is too low, it can not be effectively formed enhancing network, it is bad to the promotion of performance (comparative example 5).Adding too much
When, although can also effectively play humidification, performance has no compared with 10% and is obviously improved, therefore from cost performance isogonism
Degree considers to control additive amount lower than 10% (comparative example 6).
As can be seen that having by the graphene oxide powder that traditional stoving process obtains from embodiment 1 and comparative example 7
Higher carbon-to-oxygen ratio, this is because taking more time under forced air drying could sufficiently remove water.And this graphene oxide
Powder is existed with sheet stacking form, cannot effectively be expanded under heating condition, the performance of graphene is unable to give full play, to hair
Foam material performance contribution is little.
From embodiment 1 and comparative example 8 as can be seen that when being directly warming up to second stage when foaming, the performance of material
It is bad.This is because at relatively high temperatures, foaming agent and graphene oxide microballoon expand simultaneously, and graphene oxide microballoon is poly-
Compressed effect in polycarbonate matrix, can not effectively expand, thus while foaming agent itself can be effectively formed hole, aoxidize stone
The expansion effect of black alkene is bad, and material overall performance and pure foaming polycarbonate are close.
Claims (5)
1. a kind of graphene-foaming polycarbonate preparation method, which is characterized in that include the following steps：
(1) by atomization drying method that single-layer graphene oxide dispersion liquid is dry, graphene oxide microballoon is obtained, carbon-to-oxygen ratio is
3~6.
(2) 1~10 mass parts graphene oxide microballoon for obtaining step (1) is uniformly mixed with 1~6 mass parts foaming agent.
(3) by 100 mass parts polycarbonate and 0.1~0.6 part of stearic acid, 0.3~1 part of cumyl peroxide, 0.6~1 part
Zinc oxide, which is added in mixer, carries out mixing, and temperature is 85~100 DEG C.
(4) mixer is added together with the product of step (2) in the product of step (3), in 100~110 DEG C of mixings.
(5) mold is added in the product for obtaining step (4), foams 3~10 minutes at 120~135 DEG C, is warming up to 136~300
It foams 8~30 minutes at DEG C.
2. the method according to claim 1, wherein the atomization drying temperature of the step (1) is 130~200
℃。
3. decomposing temperature the method according to claim 1, wherein the foaming agent of the step (2) is AC foaming agent
Degree is 130~140 DEG C.
4. the method according to claim 1, wherein in the step 1 single-layer graphene oxide size be 1~
50 microns.
5. a kind of graphene-foaming polycarbonate composite material, which is characterized in that graphene film is overlapped to form porous network and is filled in
Among the hole of foaming polycarbonate.
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